A facile three-step protocol toward methoxy isoquinolines 7 starting with substituted 2- allylbenzaldehydes 9 was described. The overall synthetic process of skeleton 7 was carried out using the Grignard addition, PCC-oxidation, and one-pot oxidative cleavage of the olefinic group of skeleton 9 with OsO4–NaIO4 followed by the condensation of the resulting 1, 5-dicarbonyl compounds with NH4OAc. Skeleton 9 was prepared in high yield via the ...